西索米星原料药中极性小组分的研究

Studies on the polar minor components of sisomicin bulk material

用大孔吸附型树脂对西索米星原料药进行分离，极性小组分首先被洗脱。用高效液相色谱法测定了分离前后的西索米星纯度，发现可从８４％提高到９２％。此外还建立了用硅胶薄层层析检测小组分的方法，并用阳离子交换树脂对小组分进行了分离。采用上述方法可分离得６种小组分。再用Ａｍ－ｂｅｒｌｉｔｅＣＧ－５０、ＣＭ－ＳｅｐｈａｄｅｘＣ－２５等精制，得各小组分的精制品，经冷冻干燥后进行结构测定。其中含量最多的ＮＡＴ－１、ＵＫ－１与庆大霉素Ａ和加洛糖胺同质，ＮＡＴ－４与庆大霉素Ａ１的文献报道相符；而ＮＡＴ－２、ＵＫ－２经ＭＳ、１Ｈ－ＮＭＲ、１３Ｃ－ＮＭＲ测定。

The complex of minor components was isolated from sisomicin bulk material by macroporous adsorption resin. Then, the polar minor components were eluated first. They were separated into six components by ion exchange resin; and the purity of sisomicin increased from 84% to 92%. We performed an experimental study of the method for the identification of minor compo nents by the use of thin layer chromatography. Each minor component was purified by repeated ionexchange chromatographic processes. Finally, NAT 1 and UK 1 were identified as gentamicin A and garamine and NAT 4 was identified as gentamicin A 1by comparing with reported MS, 1H NMR and 13 C NMR data. NAT 2 and UK 1 were inferred as new pseudodisuccharides by 1H NMR, 13 C NMR and mass spectroscopic studies.